Liu Fei, Xu Yu, Rui Lei, Gao Shu, Dong Haijun, Guo Qingxiang
Department of Chemistry, University of Science and Technology of China, Hefei 230026, China.
Rapid Commun Mass Spectrom. 2006;20(23):3522-6. doi: 10.1002/rcm.2764.
A simple, rapid, sensitive and specific liquid chromatography/tandem mass spectrometry method was developed and validated to quantify troxerutin in human plasma. The analyte and rutin, used as the internal standard, were analyzed on a Phenomenex Synergi Fusion RP column interfaced with a triple-quadrupole tandem mass spectrometer using positive electrospray ionization. Acetonitrile/water (20:80 v/v) was used as the isocratic mobile phase, with 0.1% formic acid in water. A simple sample preparation method of protein precipitation with perchloric acid was employed. The assay was linear over the concentration range 31.25-4000 pg/mL. Correlation coefficients generated by linear regression with a 1/x(2) weighting factor ranged from 0.9991 to 0.9996. The intra- and inter-day precision over the entire concentration range were less than 12.28%. The method was successfully applied to a pharmacokinetic study after oral administration of a 300 mg troxerutin drop pill to 18 healthy volunteers.
建立并验证了一种简单、快速、灵敏且特异的液相色谱/串联质谱法,用于定量测定人血浆中的曲克芦丁。以芦丁作为内标物,在配备了电喷雾正离子源的三重四极杆串联质谱仪的Phenomenex Synergi Fusion RP色谱柱上对分析物和内标物进行分析。乙腈/水(20:80 v/v)作为等度流动相,水相中含有0.1%的甲酸。采用了用高氯酸沉淀蛋白质的简单样品制备方法。该测定法在31.25 - 4000 pg/mL的浓度范围内呈线性。通过具有1/x(2)加权因子的线性回归生成的相关系数在0.9991至0.9996之间。在整个浓度范围内,日内和日间精密度均小于12.28%。该方法成功应用于18名健康志愿者口服300 mg曲克芦丁滴丸后的药代动力学研究。